电感耦合等离子体原子发射光谱法测定锆合金中5种元素的含量
Determination of 5 Elements in Zirconium Alloy by Inductively Coupled Plasma Atomic Emission Spectrometry
巩琛 1黄辉 1冯典英 1张嘉祺 1李颖 1李本涛1
作者信息
- 1. 中国兵器工业集团第五三研究所,济南 250031
- 折叠
摘要
提出了电感耦合等离子体原子发射光谱法测定锆合金中锡、铌、铁、铬、镍含量的方法.取样品0.1 g,加入5 mL水、5 mL硝酸和0.5 mL氢氟酸,于100℃加热5 min,用水定容至25 mL.设置仪器射频功率为1 300 W,雾化气流量为0.80 L·min-1,进样量为2.0 mL·min-1,测定5种元素在Sn 242.949 nm、Nb 309.418 nm、Fe 259.941 nm、Ni 221.648 nm、Cr 267.716 nm等分析谱线处的响应强度,基质匹配法定量.结果表明:锡、铌的质量浓度在150 μg·mL-1以内,铁、铬、镍的质量浓度在15 μg·mL-1以内分别与对应的响应强度呈线性关系;锡检出限(3s)为16 μg·g-1,其他元素检出限(3s)均低于3.0 μg·g-1;各元素方法重复性的相对标准偏差(n=10)均小于2.0%,加标回收率为99.0%～109%;采用锆合金标准物质SRM360b进行验证,测定值均在认定值的不确定度范围内.
Abstract
A method for the determination of Sn,Nb,Fe,Cr and Ni in zirconium alloy by inductively coupled plasma atomic emission spectrometry was proposed.The sample(0.1 g)was taken,and 5 mL of water,5 mL of nitric acid and 0.5 mL of hydrofluoric acid were added.After heating at 100℃for 5 min,the volume of the mixed solution was made up to 25 mL with water.The response intensities of 5 elements at Sn 242.949 nm,Nb 309.418 nm,Fe 259.941 nm,Ni 221.648 nm and Cr 267.716 nm were determined with the radio frequency power of 1 300 W,the atomizing gas flow rate of 0.80 L·min-1,and the sample injection amount of 2.0 mL·min-1,and the matrix matching method was used for quantification.It was shown that linear relationships between mass concentration and response intensity were kept within 150 μg·mL-1 for Sn and Nb,and 15 μg·mL-1 for Fe,Cr and Ni,and the detection limit(3s)of Sn was 16 μg·g-1,and the detection limits(3s)of other elements were lower than 3.0 μg·g-1.RSD(n=10)for the method reproducibility of each element was less than 2.0%,and the spiked recoveries were in the range of 99.0%-109%.Zirconium alloy standard substance SRM360b was used for verification,and the determined values were within the uncertainty ranges of the confirmed values.
关键词
电感耦合等离子体原子发射光谱法/锆合金/元素Key words
inductively coupled plasma atomic emission spectrometry/zirconium alloy/element引用本文复制引用
出版年
2024
NETL
NSTL
万方数据